JPS58151318A - Synthetic silica and resin composition containing it for sealing electronic parts - Google Patents

Abstract

PURPOSE:To obtain synthetic silica almost free from radioactive substances and suitable for use as a filler for a resin composition for sealing electronic parts, by hydrolyzing a silicon compound purified by distillation to form polysiloxane and by heat treating the polysiloxane. CONSTITUTION:A silane compound having a hydrolyzable group such as methyltrimethoxysilane is purified by distillation and hydrolzed to form polysiloxane. The polysiloxane is dried, oxidized under heating, and pulverized to about 0.5- 100mum average particle size to obtain synthetic silica contg. <=about 10ppb uranium and thorium. About 50-800pts.wt. said synthetic silica is blended with about 100pt.wt. synthetic resin such as epoxy resin or polyphenylene sulfide resin to form a resin composition for sealing highly integrated electronic parts such as LSI and VSLI.

Description

Detailed Description of the Invention The present invention relates to synthetic silica, particularly synthetic silica which is suitable as a filler for resin compositions for encapsulating electronic components, and resin compositions for encapsulating electronic components containing the same. It is related to two things.

Electronic parts are generally made from synthetic resin compositions C; in terms of protection from the external environment and productivity. This synthetic resin composition is mainly composed of organic resin and lime. ! This composition (first of all, it has a coefficient of expansion as small as possible,
In order to achieve good thermal conductivity, low moisture permeability, excellent mechanical properties, and low cost, it is important to incorporate as much of this inorganic filler as possible in the formability of the material. It is considered advantageous. For this purpose, a silica-based filler is considered to be preferable, and most resin sealing materials are used. Each of these has advantages and disadvantages, and is used depending on the purpose and use.

On the other hand, regarding the silica filler, from the viewpoint of the above-mentioned large amount formulation, silica with a relatively large average particle size, for example, 1 to 100 μm, is used, so this book uses natural ore. Quartz powder is used, which is obtained by pulverizing natural ore without refining it, or by washing natural ore with water, treating it with hydrofluoric acid, sintering or melting it at 1000 to 1800°C, and then pulverizing it.

On the other hand, with the advancement of technology, memory elements sealed with this resin composition have become more integrated, and today they have already become highly integrated LSIs called VL8I. However, this highly integrated electronic component is sealed with resin (in addition, the resin composition is made up of a carbon filler containing a large amount of α released from radioactive elements such as uranium and thorium). MO8RA
M 17) Design etc. (: also has a big influence, so
This solution is desired. Therefore, as a countermeasure to this problem, a method has been proposed in which the surface of the memory element (=polyimide resin% silicone resin, etc.) is coated in advance to protect the element from alpha ray irradiation. The surface of the element has a certain thickness and a certain area (:
It is difficult to apply this resin, and there is also a performance concern that problems may easily occur due to the difference in expansion coefficient between the memory element, these resins, and the above-mentioned sealing resin composition. It is said that this method is not advantageous in terms of production efficiency and economy, partly because of the complexity associated with the coating process.

Therefore, the resin composition for sealing the memory element (the silica filler used on the second side) is made of various synthetic silicas currently available on the market, such as silicon tetrachloride, at a high temperature (1850 to 2000°F).
), dry silica made by flame hydrolysis with H, O, C, precipitated silica obtained by neutralizing hydrated sodium silicate with hydrochloric acid, or neutralizing with hydrated sodium silicate, alcohol. The use of silica aerogel obtained by neutralization in coexistence has also been considered, but all of these have fine particles with an average particle diameter of the order of micrometers and a specific surface area (BET method) of 50 tf/j or more. It also has a large number of lanol groups on its inner and outer surfaces, so even if it were possible to highly purify C2 so that it does not contain radioactive elements, it could be treated as an organic resin C: a large amount (= It has been confirmed that it cannot be filled and therefore cannot be used in resin compositions for encapsulating electronic components.

Additionally, it is almost impossible to completely remove residual alkali ions using hydrated sodium silicate as a starting material. Appropriate.

That is, C for electronic component sealing: High purity silica which is suitable for high filling and can be filled does not currently exist and is said to be impossible to obtain.

The present invention provides synthetic silica that can be used as a resin composition for encapsulating electronic components that can solve these disadvantages, and a resin 41 composition for encapsulating electronic components containing the same.
This is a synthesis process obtained by drying and/or heating oxidizing polysiloxane obtained by hydrolyzing silane having a hydrolyzable group purified by distillation and its derivatives polysiloxane and (poly)silazane. Ririka C
Two related I81 inventions and thermosetting resins or thermal iT! !
l-type resin 1oo*: tg+=Resin composition for encapsulating electronic components, which is formed by adding 50 to 800 parts of the synthetic silica of the first invention t: Comprises the related second invention.

Taking this into account, the present inventors discovered the above-mentioned α-ray emission (
Countermeasures against memory element malfunctions, which are called soft errors due to If we use a silicon compound of the type described above, we can convert the resulting synthetic silicon into uranium,
Synthetic silica is made from this silicon compound, focusing on the fact that it can contain almost no radioactive elements such as thorium! Please call me for further consideration.

This C: is obtained by decomposing a silicon compound by distillation and stirring into polysilochitin, which is heated to 51! The present invention was completed by discovering that it is sufficient to carry out the following steps.

The silicon compound used as the starting material for producing the synthetic silica of the first aspect of the present invention is a silane having a hydrolyzable group in its molecule and a polysiloxane, which is a derivative thereof, (
poly)silazane.

Typical examples of this hydrolyzable group include a herogen atom, an alkoxy group, an alkenyloxy group, an alkoxy group, etc., but the group is not limited to these.

For example, the silane has the formula uJs1x4-. (Here, CR is a hydrogen atom or a monovalent hydrocarbon group, X is an atom or group having hydrolyzability, and j is 0 to 3). Specifically, tetrachlorosilane (
810j4)
)% Digloro V run (H!8101.), Methyltrichlorosilane (OH,810j, )% DimethyldichloroC7f/Uy [(oH,>, 51oi, ),
Dorimechaglochinuran ((OH-,8101), Methyldichloro-a-silane (ollsslaoj, ), Phenyltrichlorosilane (0,if, 81 (M, ), Diphenyldiglomuchinuran ((0,H,), 810j, )
, phenyldichlorosilane (0,H,81HOj,),
Tetraethoxysilane (81(0OHs)4),
Methyltrimethoxysilane (0 horse 5 itoaas),)
, dimethyldimethoxysilane ((OH, 481(OOH
, ) , ), tetraethoxysilane (81(00,H,
J, ], phenyltotumethoxy ν run (o, a, 5t (
oaa, ), ), dimethyljethoxysilane ((OHs
)
), ), etc., which can be used alone or as a mixture of two or more.

Furthermore, polysilochitin, which is a derivative of two-chain silane, has an average composition formula (% formula % (where CR' is a hydrogen atom, a -valent hydrocarbon group or a hydrolyzable group, and n is 1.2 to 2-3). There are no restrictions on the structure of the skeleton, degree of polymerization, etc. for these two polysiloxanes.

It may be oil-like, rubber-like or varnish-like.

Examples of such polysiloxanes include those of the formula (OH, 8
10: ) Various types can be used, including polysilochitin, which is represented by n (where Cn is an arbitrary number) and whose terminal group is a methoxy group.

In addition, (water 9) silazane is represented by the formula 1 (where R is a hydrogen atom, a -valent hydrocarbon group, or a hydrolyzable group, m is O or a positive integer), and C
; It is essential that it has one or more hydrolyzable groups.

Such polysilazane can be synthesized by a conventionally known method (2).
81N (OA) 81 (OH,), .

(OH,), SiN'H ((OH,), 81NH)
81 (OH,).

etc. can be given.

381-0- can be prepared by conventional methods, such as hydrolysis in acidic or alkaline aqueous solutions.
816, which becomes polysiloxane by condensation, but can be crushed and/or dispersed to have various particle size distributions. In this case, in order to obtain polysilochitin powder with a large particle size, the above-mentioned silane is partially dihydrolyzed and condensed to increase the degree of polymerization.

Alternatively, hydrolysis may be carried out in the coexistence of a hydrophilic solvent, but the particle size is determined by the hydrolysis conditions 1, such as the hydrolysis temperature, the acidity or basicity of the water used for hydrolysis, and the strength of stirring (: In general, the higher the hydrolysis temperature and the greater the stirring intensity, the smaller the particle size of bosslochitin becomes. However, in the case of carrying out the present invention, when the water decomposition temperature is 1-10°C or lower, the rate decreases. However, if a silicon compound with a low boiling point is used at temperatures above 100°C (- some of which hydrolyze in the gas phase and the resulting polysilochitin has a fine particle size (2), this
The temperature range is from 10°C to 100°C, preferably from 20 to 80°C.

The polysilochitin obtained by this hydrolysis C2 is dried and/or heated and oxidized, and then crushed or classified. In this case, bosslochitin becomes organobolisia chitin, which is preferably heated to oxidatively cleave its parent groups to form the final silica, which does not contain any parent groups at all. It may also be partially heated and oxidized to contain an organic group. Among these silanes, OH, 810j, which is considered to be one of the useful starting materials, is relatively poorly utilized in the current silicone industry.
It is suitable for its effective use. OI in the silane
is hydrolyzed C: Therefore, it is recovered as HOJ, and the gel-like substance produced has a lower Oj content than washing C2, but it is also thermally decomposed at a high temperature of 100°C or more for a long time, and is converted into methyl groups ( = Easily removed by C dioxide.

Also, when %OH, 5iOj, is alkoxylated, for example, OH
, 81 (OOH, -), 01 minutes may be removed, hydrolyzed to gel, washed and dried; in this case, (
- indicates the ability to leave the methyl group and use it as a hydrophobic synthetic resin.

Furthermore, in the CS of the present invention, solvent-soluble bosslochitin and (poly)V-radene are synthesized in advance, hydrolyzed to gel, and then dried and heated to oxidize in the same manner as described above.C: Accordingly, synthetic silica can also be obtained.

The raw material for the uranium, i/9, obtained by C Niji is distillation rod.
The content of radioactive elements such as thorium is 10 ppb or less,
In particular, the content of alkali metal ions such as Na, etc., which causes deterioration in moisture resistance of resin compositions made using this as a filler and corrosive properties of aluminum, has been reduced to a trace level. The amount is extremely low, which is special
2. It is suitable as a filler constituting the resin composition for encapsulating electronic components described above.

In the above-mentioned method (:), by appropriately selecting the conditions, it is possible to obtain particles having a particle size that can be directly applied to the sealing resin composition without any pulverization, and therefore does not require a pulverization step. In this case, there are no disadvantages such as contamination of CVM power during the process or not necessarily advantageous in terms of purity.

When used for this purpose, if the average particle size of this synthetic silica is less than 0.5μ, the fluidity and moldability of this resin composition will deteriorate, and if it is more than 100/II, it will be difficult to form during molding. Since there is a possibility that the gate of the molding machine may become clogged, it is preferable to set the value in the range of 0.5 to 100 μm.

Electronic component encapsulation suspension bridge nui7 as a second invention of the present invention is obtained by blending this synthetic silica with a thermosetting resin or thermoplastic resin (-), which is conventionally used as a resin for encapsulating electronic components. Examples of C: include epoxy resin% silicone, thermosetting resins such as epoxy resin, silicone resin, polyimide resin, and thermoplastic resins such as polyphenylene thylphide resin.

This silicone resin has the formula R81X, (here CR
% or the same as above, TJI position constituents and formula R, 8iX,
(R and X are the same as above, DI7II-position constituents)
V run mixture 41 mainly composed of organosilane shown in
) It can be synthesized by a conventional method of co-hydrolysis in the coexistence with an organic solvent such as toluene, xylene, alcohol or acetate.

Of course it is necessary (for example, even if it has a T or D structure depending on the case) z%'5toJs%O6H, 8101
゜ or (0, H,), 810j,, (OH,), 8
10J,,OH,-,810j.

It is also possible to use Noriran of C2 or higher, such as. Generally, resins with a T unit content of 70% or more and a large number of functional groups (28i-OH) are suitable for the present invention.

Moreover, a multi-block polymer consisting of T unit blocks and D unit blocks represented by ÷TxDy may be added to this silicone resin-2 as a flexibility imparting agent.

The curing of the silicone resin is described, for example, in Japanese Patent Publication No. 43-3020.
As disclosed in No. 2, by utilizing the condensation reaction of C dilead compound and lanol groups, or by introducing some of the organic groups in the above-mentioned resin C: unsaturated groups such as vinyl groups and hydrogen atoms. , PT, a method using an addition reaction using an addition reaction catalyst such as a PT compound, etc. :@A as shown
It is also possible to adopt a method of curing using a catalyst.

Moreover, this epoxy resin has at least two
Those having 5 epoxy groups are used.

Examples of this include those synthesized from epichlorohydrin and bisphenols and various novolak resins, alicyclic epoxy resins, and epoxy resins into which halogen atoms such as Oj and Br7;j are introduced. In addition, curing agents for this resin include diaminodiphenylmethane, diaminodiphenylsulfone, metaphenylenediamine, etc.; representative amine-based curing agents; and acid anhydride-based curing agents such as phthalic anhydride, pyromellitic anhydride, and benzophenonetetracarboxylic anhydride. A curing agent or a novolac curing agent having 22 or more hydroxyl groups in one molecule, such as phenol novolac resin or cresol novolac resin, can be used, but C2 is imidazole or its derivatives. A curing accelerator such as a tertiary amine derivative, a phosphic acid derivative, or the like may be added.

Furthermore, as this polyimide resin C1, those conventionally used for sealing electronic components can be used.

This thermoplastic resin, polyphenylene thylphide resin, has the highest heat resistance among thermoplastic resins in which pechene rings obtained by the reaction of p-diglolopene and N-methylpyrrolidone are linked with sulfur atoms. This material has the characteristics of low moisture permeability, chemical resistance, and flammability, and has excellent dimensional stability, so it is suitable for sealing C-2 parts like the silicone resin and epoxy resin mentioned above. It is said to be useful as a.

In addition, when these resins mentioned above are used as a composition of the present invention, this composition must particularly prevent the emission of alpha rays, so this one prerequisite is It is best to remove impurities as much as possible, and therefore, remove unreacted monomers, hydrolyzable ^rogens, and ionic impurities such as (== Na and C) so that they are within a certain limit. : Preferably purified.

The resin composition for encapsulating electronic components of the present invention can be obtained by blending the organic resin described above and the synthetic resin described above. This can be done using a machine etc.

The blended amount of synthetic V9 force lowers the expansion coefficient of this composition, and this effect is not fully achieved with C: 100% of organic resin, so this is 50 to 50% of synthetic quartz powder to 100 parts of organic resin. It is preferably in the range of 800 coulometric parts, particularly from 100 to 500 coulometric parts.

In addition, this composition may contain various additives, such as a silicon compound having a leprosy group such as an epoxy group and a hydrolyzable atom or group such as a hydroxyl group in one molecule. Good too. This compound is commonly referred to as a carbon functional silane or polyloxane. The hydrolyzable atom or group may include alkoxy groups, acyloxy groups, etc., but in the present invention, alkoxy groups,
A methoxy group is particularly preferred, and a hydroxyl group is also preferred.

Regarding this optional component, the silicon compound ≦;

When the main component constituting the sealing resin composition is a silicone-dipoxy resin, C: is preferably an epoxy group, and when it is a polyphenylene sulfide resin, C: is an epoxy group and an amino group. adduct is good.

Synthetic silica obtained by the above-mentioned method (2) has poor surface activity (C), hydrophilicity, and is easily wetted by water, except by simple drying of a gel that is a hydrolyzate of monoalkylsilane. However, by adding this optional component, the bonding strength between the thermosetting or thermoplastic resin and the metallic silica can be increased, and the optional component can also impart the effect of making the synthetic silica hydrophobic.

Therefore, it is particularly preferable for the silicon compound to have an organic group such as a methyl group, ethyl group, or propyl group in addition to the carbon functional group in its molecule, since this improves the water resistance of the compound.

Examples of such silicon compounds include the compounds shown to the queen.

H,HOH,OH,OH,81(00,H,),,NO
H! O horse 0 bird s i (00,H,), sOHOOH
Oh.

ss This silicon compound is used in an amount of 10 parts by weight or less, preferably 0.1 to 10 parts by weight, more preferably 0.5 to 3 parts by weight, based on 100 parts by weight of the resin. Even if it is added, it is difficult to expect the desired effect if it is less than 0.1 part by weight, and conversely, if it is more than 10 parts by weight, not only will it not be possible to obtain the effect of increasing the quantity, but also the surface of the synthetic resin ζ2rJ&
This is because the unattached surplus component C=52 appears to have an adverse effect on moldability and physical properties.

In addition, a small amount of various types of fillers such as silica silica, alumina, and ellipsoidal titanium oxide may be added to the material as long as the flow characteristics are not impaired. It is necessary to thoroughly examine and ensure that radioactive elements are not introduced into these additions.

The resin composition of the present invention described above can be shaped into an appropriate shape after being blended;
However, the sealing of electronic components can be performed by any of the conventionally known injection molding, injection molding, compression molding, and transfer molding. The effect is that it is possible to easily obtain a resin-sealed electronic component that does not cause any occurrence of.

Next, C: Examples of the present invention will be given, and all parts in the steel indicate parts by weight.

Example 1 (Extreme preparation of synthetic silica) Disilane in methyltrimeth purified by distillation at 102-103°C (boiling point 102-103°C/740 mmHg) C
Add 100 parts of Hs81 (OCHs) to 20 parts of ion-exchanged water.
After dissolving in a mixture of 0 parts and 11220 parts of vinegar, 5
The mixture was hydrolyzed at 0° C. for 5 hours to obtain bulk methylpolysiloxane. Next, the K is pulverized to form a powder with an average particle size of 10011 or less.
, 800°C, 1000°C, and 1200°C for 2 hours each.

The methyl group of O41o was oxidized to obtain white synthetic silica containing no methyl group (synthetic silica).

Next, when we checked the purity of this synthetic silica, we found that the content of uranium, thorium, etc. was about the same as that of sputum traces, and the content of uranium, thorium, etc.
, KO amount is less than several ppm, C4 ion is 10 ppm
Met.

(Preparation of sealing composition) 1) 57.5 parts of cresol novolac epoxy resin,
To an epoxy resin composition consisting of 12.5 parts of phenol novolac resin 3α411S,/L'sol novolac/brominated epoxy resin, 230 parts of the synthetic silica obtained above and 5 parts of antimony trioxide.

5 parts of 3-glycidoxyprobyl trime Foxysilone, 5 parts of carnauba wax, 5 parts of carbon black, and 4.5 parts of triphenylphosphine as a curing accelerator were added and thoroughly kneaded with two heated rolls. , and pulverized to obtain a resin composition for inhibiting electronic components-■.

2) Organic group/81 atoms=to5% methyl group/phenyl group=12. To 100 parts of phenylmethylpolysiloxane having 45% of hydroxyl groups bonded to silicon atoms, 250 parts of the synthetic silica A obtained above, 5 parts of calcium stearate α as a mold release agent, 8 parts α of lead carbonate as a hardening agent, and 5 parts of benzoic acid. The mixture was kneaded using two heated rolls and then ground to obtain a resin composition for encapsulating electronic components.

3) 100 parts K of polyphenylene sulfide resin.

200 parts of the synthetic silica obtained above and 5 parts of disilane in 3-glycidoxyglobilmeth were mixed and pelletized using an extruder to prepare a resin composition for hooking electronic parts.

In addition, this composition was tested at 510°C using a Koka Type 74-meter, with a die diameter of 1uφ x 10mm, and a load of J111.
When the apparent melt viscosity was measured at 0 kg, it was 5
It was oo boys.

4) Instead of the synthetic silica in the above-mentioned resin composition for attaching electronic parts to IK, natural silica stone, which is currently used as a filler in resin compositions for attaching electronic parts on the market, is used as filler. !
Using fused silica RD-8 (Taramori Co., Ltd., trade name), a resin composition for encapsulating electronic parts was prepared in the same manner.

(Evaluation of bone properties of resin composition for encapsulating electronic components) Regarding the resin composition for encapsulating electronic components obtained above -■~NK, its uranium,
When the thorium content, C-ray strength, fluidity 1 bending strength and volume resistivity were measured, the results shown in the table below were obtained. It was confirmed that there were no particular problems regarding physical properties.

Semi-thermal steel II! Example 2 Methyltrichlorosilane purified by distillation at 66-67℃ (
CH, 5IC11) (boiling point 60-67℃/760ma+
A mixture of 80 parts of Hg) and 20 parts of dimethyldichlorotane ((CHs)ss lC1g) purified by distillation at yo~71°C (boiling point 70~71°C/740mmHg),
The mixture was added dropwise over 1 hour to 55% hydrochloric acid water heated to 40 to 50°C, and then kept at this temperature for another 1 hour to carry out cohydrolysis. After the reaction was completed, the resulting precipitate was filtered, washed with water, and neutralized. When the precipitate obtained was dried, the average particle size was 10.
A powder of 0 μm or less was obtained.

Next, this powder was placed in a crucible and heated to 450°C.

600℃% When heated at 1000℃ and 1200℃ for 2 hours each, the methyl groups of this powder were oxidized and became white silica powder (synthetic silica B).When the purity of this powder was compared, it was found that The uranium and thorium content of the O material is n7PPb, and the Na content is 8 ppm or less.

The Cl ion content was 10 ppm.

Next, this synthetic silica B was used in place of the synthetic silica used in the resin composition for encapsulating electronic components-I in the previous example, and treated in the same manner to produce a resin composition for encapsulating semiconductor elements-■. When I investigated its physical properties, I found that
This is the C-line intensity (LOOO is hereinafter referred to as Suairal/
70-28 inches.

The song had a strength of 14 kg/2 and a volume resistivity of 1×10 11 Ω.

Example 3 gA Example 2 20 parts of the obtained synthetic silica powder was converted into a reaction product of t5-bis(p-aminophenylthiobutyl)-tetramethyldisiloyasane and benzophenonato dicarboxylic dianhydride. Sili;-boriamic acid precursor O
N-methylbiuridone solution (nonvolatile content 20%) 500
11 to make a coating material, which was used to form a thickness of 50±1071 cm on the surface of glass 72, and then heated at 100°C, 180°C, and 250°C for 2 hours each.
Then, when heated at 550°C for sO minutes, the K and O
The coating was cured.

Next, when the uranium and trichum contents of this cured coating film were examined, they were found to be less than α02 ppb, and the amount of SOG radiation emitted was less than α0001 as-·h.

Example 4 (Manufacture of synthetic silica) Synthetic silica of type 411 was synthesized in the following manner.

Charge 16916 hydrochloric acid aqueous solution to the reaction vessel.

(4 times the amount of CHslilCls K), and C
HJ81C41 was gradually added dropwise while stirring.

After the dropwise addition was completed, stirring was continued at 60° C. for 1 hour. The gel-like material produced here was separated in a furnace and washed again with ion-exchanged 80° C. OII water to make it weakly acidic. Next, add 15 gel-like substances.
Dry at 0°C to remove moisture.

When this was placed in a crucible and ignited for 10 hours in an electric furnace (final ignition temperature 1200°C), white powdery synthetic silica was obtained (synthetic silica C).

In the same reaction vessel as above, 109! Prepare hydrochloric acid aqueous solution (
81 (OCmH
s) After gradually dropping a, CH181 (OCRs) and 01:1 mixture, it was treated in the same manner as the above synthetic silica C0 synthesis, and then ignited for 6 hours, resulting in an average particle size of L5.
A synthetic silica in the form of a white powder having a micro-color was obtained (synthetic silica D).

% 15% cm(OH)s aqueous solution (4 times the amount of siloxane) was charged in the same reaction vessel as above (4 times the amount of siloxane), the end group was 10CH3, and n was! 1 to 50 mixture) was gradually added dropwise (maintained at IN! 5°C or lower), treated in the same manner as for the synthesis of synthetic silica C, and then ignited for 16 hours. Silica was obtained (synthetic silica g).

Semi-control product (manufacture of molding compound) Cresol Novotsuku Epoxy resin (trade name: EOCN-
102. Ciba Geigy) 100 parts, phenol novolac resin 60 parts, synthetic silica C to E5 synthesized above
50 copies.

A mixture consisting of 2 parts (epoxy group-containing silica xane), 12 parts of 2-methylimidazole, and 12 parts of Karna 38772719% was kneaded on a heated roll for 10 minutes, taken out in the form of a sheet, and then crushed to form a sealing composition. Prepared.

On the other hand, for comparison purposes, the same amount of commercially available silica (melted natural silica) was used instead of synthetic silica, and 5-glycidoxypropyltrimethoxysilane (commercially available product) was used instead of efflorescence-containing silica xane. A sealing composition having the same composition as above was treated in the same manner except that the same amount of KBM-405 (manufactured by Shin-Etsu Chemical Co., Ltd.) was used to obtain a sealing composition.

Regarding the sealing composition obtained above, %F was molded at 175°C for 2 minutes using a transfer molding machine, and then heated to 180°C after molding.
I did a 4hr post cure.

When the O1m strength and volume resistivity of the molded product obtained here were examined, the results shown in the table below were obtained.

Electric couple thermosteel PCT; 120℃, 2 & 9 / image, 24 hours in water vapor, page 1 continuation 0 Inventor Shin-Etsu Chemical Co., Ltd. Silicone electronic materials, 2-13-1 Isobe, Kuriyama Shuan Naka City Inventor: Shin-Etsu Chemical Co., Ltd., Silicone Electronic Materials Technology Laboratory, 1-2-13-1 Isobe, Koanka-shi, Kodamaya, Japan, 1981, Commissioner of the Japan Patent Office, Haruki Shimada, 1, Indication of the case, 1988 Patent application No. 29882 2, Title of the invention 3, Relationship with the case of the person making the amendment Patent applicant name (206) Shin-Etsu Chemical Co., Ltd. 4, Agent address Nagai, 4-9 Nihonbashi Honmachi, Chuo-ku, Tokyo 103 Pill [Telephone Tokyo (270) 085 g, 086
9) 3 6. "Detailed Description of the Invention" in the specification to be amended /--1 ゝ\l) "N-Methylpyrrolidone" in the bottom two lines of page 18 is amended to "soda sulfide."

2) On page 21, line 8, "If..., then an epoxy group and ---" is one song. If... then ζ: is an amino group or an epoxy group... ” he corrected.

3) The descriptions in lines 1 to 3 of the table on page 28 are corrected as follows.

4) In the table on page 33, in the column for commercially available silica, correct the row (7) r650J for uranium content (ppb) to "65".

Claims (1)

[Claims] 1. Synthesis obtained by drying and/or thermal oxidation of polysiloxane obtained by hydrolyzing distillation-purified silane having a hydrolyzable group and its derivatives, polysilochitin and (poly)silazane. Silica 2, Synthetic silica 3 according to Claim 1, which is dried and/or heated and oxidized, then crushed and dispersed to have an average particle size of 0.5 to 100 pores, Content of uranium and thorium. is 10 ppb or less of the synthetic silica 4 according to claim 1, and 100 parts by weight of a thermosetting resin or an island plastic resin,
Drying 2 and/or addition I of polysilochitin obtained by hydrolyzing distillation-purified silane having a hydrolyzable group and its derivatives, (poly)silazane
Resin composition 5 for encapsulating electronic components, characterized in that 50 to 800 parts by weight of synthetic V resin obtained by Il&oxidation is added, the thermosetting resin is epoxy V resin, silicone resin, epoxy-silicone resin or The composition 6 according to claim 4 is a polyimide resin, and the composition 6 is a polyphenylene nalphide resin! Composition described in Section J4